WO2020177257A1 - 一种红光及近红外发光材料、制备方法及发光器件 - Google Patents

一种红光及近红外发光材料、制备方法及发光器件 Download PDF

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WO2020177257A1
WO2020177257A1 PCT/CN2019/095238 CN2019095238W WO2020177257A1 WO 2020177257 A1 WO2020177257 A1 WO 2020177257A1 CN 2019095238 W CN2019095238 W CN 2019095238W WO 2020177257 A1 WO2020177257 A1 WO 2020177257A1
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light
red
infrared
emitting
luminescent material
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PCT/CN2019/095238
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English (en)
French (fr)
Chinese (zh)
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陈晓霞
刘元红
刘荣辉
薛原
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有研稀土新材料股份有限公司
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Priority to KR1020207037507A priority Critical patent/KR102580962B1/ko
Priority to US17/254,224 priority patent/US11932790B2/en
Priority to JP2020572811A priority patent/JP7073542B2/ja
Priority to EP19917562.1A priority patent/EP3795654B1/en
Publication of WO2020177257A1 publication Critical patent/WO2020177257A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
    • C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
    • C09K11/681—Chalcogenides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/62—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing gallium, indium or thallium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7708—Vanadates; Chromates; Molybdates; Tungstates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G15/00—Compounds of gallium, indium or thallium
    • C01G15/006—Compounds containing, besides gallium, indium, or thallium, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7776—Vanadates; Chromates; Molybdates; Tungstates
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
    • H01L33/502—Wavelength conversion materials
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008—Processes
    • H01L2933/0033—Processes relating to semiconductor body packages
    • H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements

Definitions

  • the invention relates to the field of luminescent materials, in particular to a red and near-infrared luminescent material, a preparation method and a light-emitting device.
  • the application of near-infrared light in the fields of security monitoring, biometrics, 3D sensing, and food/medical testing has become a focus at home and abroad.
  • the broad spectrum of 650nm ⁇ 1050nm covers the frequency doubling and combining characteristic information of hydrogen-containing groups (O-H, N-H, C-H) vibration.
  • the characteristic information of the hydrogen-containing groups of organic molecules in the sample can be obtained, which can be widely used in the field of food detection.
  • Broad spectrum or multi-spectrum of 850-1000nm and 1400-1700nm can be applied to the fields of medical detection, biometric identification and security monitoring.
  • the patent "Near infrared doped phosphors having an alkaline gallate matrix” discloses that the composition is LiGaO 2 : 0.001Cr 3+ , 0.001Ni 2+ , which can produce near-infrared luminescence between 1000nm and 1500nm under ultraviolet light excitation.
  • the spectral range is narrow, the luminous intensity is low, and the phosphor has a long afterglow effect, and the luminous time lasts for several minutes, which is not suitable for light-emitting devices.
  • the problem to be solved by the present invention is the deficiencies of the above-mentioned luminescent materials.
  • One of its objectives is to obtain a red and near-infrared luminescent material and a preparation method thereof. Compared with the existing red and near-infrared luminescent materials, the material has It can be excited by a spectrum with a rich wavelength range (ultraviolet or violet light or blue light) to produce 650nm ⁇ 1700nm broad spectrum or multiple spectrum light.
  • another object of the present invention is to provide a device that uses a single excitation light source and uses the luminescent material of the present invention to generate red light and near-infrared light in the range of 650 nm to 1700 nm.
  • the present invention proposes a red light and near-infrared light-emitting material, a preparation method thereof, and a light-emitting device containing the material.
  • a first aspect the present invention provides a red and near-infrared light emitting material, the emissive material comprises the formula aSc 2 O 3. Ga 2 O 3. Compound bR 2 O 3, wherein said R element comprising Cr, Ni One or two of, Fe, Yb, Nd or Er elements, 0.001 ⁇ a ⁇ 0.6, 0.001 ⁇ b ⁇ 0.1.
  • the compound has the same crystal structure as ⁇ -Ga 2 O 3 .
  • the R element includes Cr.
  • the R element is Cr.
  • the R element also includes one or two of Ce, Eu, Tb, Bi, Dy, and Pr.
  • the second aspect of the present invention provides a method for preparing the aforementioned red light and near-infrared luminescent materials, including the following steps:
  • the sample is ball milled, washed with water and sieved to obtain the red and near-infrared luminescent materials.
  • the third aspect of the present invention provides a light emitting device, which includes at least an excitation light source and a light emitting material, and the light emitting material at least includes the red light and near-infrared light emitting materials as described above.
  • the peak wavelength range of the excitation light source is 250-320nm, 400-500nm and 550-700nm.
  • the emission peak wavelength range of the excitation light source is 440-470 nm.
  • the present invention provides a material and a light-emitting device that can generate red light and near-infrared light with high intensity and broad spectrum or multiple spectra.
  • the luminescent material can be excited by ultraviolet, blue and red light sources to generate a broad spectrum or multiple spectra.
  • the luminescent material can be excited by a mature blue light source to produce high-intensity broad spectrum or multiple spectrum luminescence, which has higher luminous intensity than existing materials.
  • Fig. 1 is an XRD diffraction pattern of the luminescent material obtained in Example 1 of the present invention
  • Example 2 is an excitation emission spectrum diagram of the luminescent material obtained in Example 1 of the present invention.
  • Fig. 3 is an excitation emission spectrum diagram of the luminescent material obtained in Example 2 of the present invention.
  • a first aspect the present invention provides a red and near-infrared light emitting material, the emissive material comprises the formula aSc 2 O 3. Ga 2 O 3. Compound bR 2 O 3, wherein said R element comprising Cr, Ni One or two of, Fe, Yb, Nd or Er elements, 0.001 ⁇ a ⁇ 0.6, 0.001 ⁇ b ⁇ 0.1.
  • said aSc 2 O 3. 2 O 3 Compound bR 2 O 3, Ga has the same ⁇ -Ga 2 O 3 crystal structure. Ga 2 O 3 has five allotropes ⁇ , ⁇ , and ⁇ . Among them, ⁇ -Ga 2 O 3 is the most stable. It has a monoclinic crystal structure and is chemically stable and easy to dope with cations. . In the present invention, ⁇ -Ga 2 O 3 can realize red light and near-infrared light emission by introducing transition metal or rare earth metal ions. In addition, the tunable and controllable spectrum can be achieved through the substitution of other elements of the same group.
  • a and b further have a value range: 0.15 ⁇ a ⁇ 0.35, 0.02 ⁇ b ⁇ 0.05.
  • the red and near-infrared luminescent material of the present invention is characterized in that ⁇ -Ga 2 O 3 is doped with Sc element, which has a larger atomic radius and replaces Ga cations, which expands the lattice of ⁇ -Ga 2 O 3 and emits central ion and anions O bond length becomes long, thereby promoting crystal field strength weakens or crystal field splitting, Cr ions to achieve broadband or multi-spectral emission, and with the increase of the content of Sc ions, to achieve long-wave spectral movement, when Sc 2 O When the content of 3 is 0.15 ⁇ a ⁇ 0.35, the luminescent material of the present invention has a ⁇ -Ga 2 O 3 structure and has a higher luminous intensity.
  • the luminous intensity When a is less than 0.15, the luminous intensity is slightly lower, and when a exceeds 0.35, impurities may be generated. phase.
  • the R element in R 2 O 3 is used as the luminous center.
  • the composition is 0.02 ⁇ b ⁇ 0.05, the luminescent material of the present invention has the best luminous intensity.
  • b ⁇ 0.02 because there are too few luminous centers, the luminous intensity is low, when b> 0.05, too high a concentration of the luminescent center will cause concentration quenching, which will also reduce the luminous intensity.
  • the R element includes Cr.
  • the R element is Cr.
  • the transition metal ion Cr 3+ has a radius similar to that of Ga 3+ , and is easily doped into the twisted octahedral structure of Ga 3+ , and the energy level of Cr 3+ can decrease as the crystal field strength becomes weaker. , Can realize the long-wave shift of the spectrum and obtain the broad peak emission, thereby producing near-infrared broad spectrum luminescence.
  • the red light and near-infrared light-emitting materials also include one or two of Ce, Eu, Tb, Bi, Dy, and Pr.
  • the introduction of one or two of the elements Ce, Eu, Tb, Bi, Dy, and Pr can cause the energy transfer of this type of element to the central element R to obtain stronger red light and near-infrared light.
  • the second aspect of the present invention provides a method for preparing the above-mentioned red light and near-infrared luminescent material, which includes the following steps:
  • the sample is ball milled, washed with water and sieved to obtain the red and near-infrared luminescent materials.
  • the third aspect of the present invention provides a light-emitting device, which can be made into a light-emitting device using the aforementioned red light and near-infrared light-emitting materials in combination with an excitation light source.
  • the excitation light source has a peak wavelength range of 250-320nm, 400-500nm, 550-700nm, preferably 440-470nm.
  • the stoichiometric ratio of the chemical formula Sc 0.98 BO 3 :0.02Cr accurately weigh Sc 2 O 3 , H 3 BO 3 and Cr 2 O 3 and mix them uniformly to obtain a mixture; the obtained mixture is calcined at 1300°C for 8 hours in an air atmosphere, The calcined product is obtained after cooling; the obtained calcined product is subjected to post-processing such as sieving and water washing to obtain a near-infrared luminescent material sample.
  • the obtained near-infrared luminescent material sample was subjected to a 460nm excitation test, and it was obtained that the emission peak of the comparative example was located at 810nm, the half-value width was 133nm, and the relative luminescence intensity was set to 100.
  • Example 1 11-0370 ⁇ -Ga 2 O 3 , except for the overall diffraction The peak shifted slightly to a small angle, indicating that the structure of Example 1 was ⁇ -Ga 2 O 3 structure.
  • the introduction of Sc element resulted in a ⁇ -Ga 2 O 3 Sc-doped solid solution, and its crystal lattice expanded. The surface spacing increases.
  • the luminescent material obtained in Example 1 was analyzed by a fluorescence spectrometer, and the luminescence spectrum was obtained by excitation at blue light at 460nm.
  • the material has broad-spectrum luminescence of red light and near-infrared spectrum under blue light excitation, reaching 650nm ⁇ 1050nm, and its peak The wavelength is 798nm, the half-peak width is 141nm, and the excitation spectrum is obtained by monitoring its 798nm emission, as shown in Figure 2. It can be seen that the luminescent material can be effectively excited by ultraviolet, violet, blue and red light, emitting a broad spectrum of red light and near-infrared light. Its relative luminous intensity is 309.
  • the luminescent material obtained in Example 2 was analyzed by a fluorescence spectrometer, and the luminescence spectrum was obtained by excitation at 460nm of blue light.
  • the material has broad-spectrum luminescence of red light and near-infrared spectrum under blue light excitation, reaching 650nm ⁇ 900nm, and its peak The wavelength is 734nm and the half-peak width is 121nm. Monitor the 734nm luminescence to obtain the excitation spectrum, as shown in Figure 3. It can be seen that the luminescent material can be effectively excited by ultraviolet, violet, blue and red light, emitting a broad spectrum of red light and near-infrared light. Its relative luminous intensity is 245.
  • the luminescent material obtained in Example 3 was analyzed by a fluorescence spectrometer, and the luminescence spectrum was obtained by excitation at 460nm of blue light.
  • the material has broad-spectrum luminescence of red light and near-infrared spectrum under blue light excitation, reaching 700nm ⁇ 1050nm, and its peak The wavelength is 830nm, the half-peak width is 143nm, and its relative luminous intensity is 258.
  • the compound composition formulas are listed in Table 1 below.
  • the preparation method of the materials in each embodiment is the same as that in Example 1, and only needs to be based on the target in each embodiment.
  • the chemical formula composition of the compound select the appropriate amount of the compound, mix, grind, and select appropriate firing conditions to obtain the required near-infrared luminescent material.
  • the luminescent material of the present invention has the characteristics of broad-spectrum emission or multi-spectrum emission of red light and near-infrared light under blue excitation. Compared with the existing near-infrared luminescent materials, the comparative example is used for comparison. The invented red and near-infrared luminescent materials have higher luminous intensity.
  • the present invention provides a near-infrared and red light emitting material and its preparation method, and a light emitting device comprising the light emitting material, the red and near-infrared light emitting material comprising the formula aSc 2 O 3. Ga 2 O 3. compound bR 2 O 3, wherein R comprises one or two elements of Cr, Ni, Fe, Yb, Nd or Er elements, 0.001 ⁇ a ⁇ 0.6,0.001 ⁇ b ⁇ 0.1.
  • the luminescent material can be excited by a spectrum with a rich wavelength range (ultraviolet or violet light or blue light) to produce 650nm-1700nm broad spectrum or multiple spectrum luminescence, and has higher luminous intensity.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
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  • Computer Hardware Design (AREA)
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PCT/CN2019/095238 2019-03-06 2019-07-09 一种红光及近红外发光材料、制备方法及发光器件 WO2020177257A1 (zh)

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KR1020207037507A KR102580962B1 (ko) 2019-03-06 2019-07-09 적색광 및 근적외선 발광재료, 제조 방법 및 발광소자
US17/254,224 US11932790B2 (en) 2019-03-06 2019-07-09 Red light and near-infrared light-emitting material, preparation method thereof and light-emitting device
JP2020572811A JP7073542B2 (ja) 2019-03-06 2019-07-09 赤色光・近赤外発光材料、その調製方法、および発光デバイス
EP19917562.1A EP3795654B1 (en) 2019-03-06 2019-07-09 Red and near-infrared light-emitting material, preparation method therefor and light-emitting device

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CN201910169021 2019-03-06

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CN112831321A (zh) * 2019-11-22 2021-05-25 亿光电子工业股份有限公司 荧光材料及光电子器件
CN111739988B (zh) * 2020-06-29 2021-11-12 山东大学 一种垂直结构宽带近红外led及制备方法
JP7491811B2 (ja) * 2020-10-28 2024-05-28 株式会社日立ハイテク 蛍光体、それを用いた光源、生化学分析装置、及び蛍光体の製造方法
CN113004896B (zh) * 2021-03-10 2023-04-07 江西离子型稀土工程技术研究有限公司 一种近红外发光材料、制备方法以及一种发光装置
CN114806564B (zh) * 2022-03-18 2024-01-12 佛山科学技术学院 三价铬离子掺杂氟锑酸盐近红外荧光材料、制备方法及其led光源
CN116161949B (zh) * 2022-12-30 2024-04-16 岭南现代农业科学与技术广东省实验室茂名分中心 一种Ga2O3:Cr3+掺杂近红外陶瓷发光材料的制备方法及其应用
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